A sensitive spectrophotometric method for the determination of trace amounts of cobalt based on the complex formation with nitrosochromotropic acid in ammoniacal medium is described. After its extraction as thiocyanate complex into isobutylmethyl ketone, cobalt is stripped into nitrosochromotropic acid in ammonia buffer. The method has been applied to the determination of cobalt in mild steel, ferrous alloys and multivitamin preparations.